#------------------------------------------------------------------------------
#$Date: 2021-02-05 16:53:19 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261799 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022288.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2022288
loop_
_publ_author_name
'Rosiak, Damian'
'Okuniewski, Andrzej'
'Chojnacki, Jaros\/law'
_publ_section_title
;
The influence of the type of halogen substituent and its position on the
molecular conformation, intermolecular interactions and crystal packing
for a series of 1-benzoyl-3-(halogenophenyl)thioureas
;
_journal_coeditor_code WP3011
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 11
_journal_page_last 19
_journal_paper_doi 10.1107/S2053229620015594
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C14 H11 I N2 O S'
_chemical_formula_moiety 'C14 H11 I N2 O S'
_chemical_formula_sum 'C14 H11 I N2 O S'
_chemical_formula_weight 382.21
_chemical_name_common 1-Benzoyl-3-p-iodophenylthiourea
_chemical_name_systematic
;
1-Benzoyl-3-(4-iodophenyl)thiourea
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 61.622(7)
_cell_angle_beta 86.203(9)
_cell_angle_gamma 85.241(9)
_cell_formula_units_Z 2
_cell_length_a 4.4279(5)
_cell_length_b 13.0767(14)
_cell_length_c 13.4410(14)
_cell_measurement_reflns_used 17633
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 29.63
_cell_measurement_theta_min 3.00
_cell_volume 682.06(14)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'Stoe IPDS 2T'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0202
_diffrn_reflns_av_unetI/netI 0.0201
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 9681
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.000
_diffrn_reflns_theta_min 3.001
_exptl_absorpt_coefficient_mu 2.493
_exptl_absorpt_correction_T_max 0.9317
_exptl_absorpt_correction_T_min 0.7340
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2009), by Gaussian integration,
analogous to Coppens (1970)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.861
_exptl_crystal_description needle
_exptl_crystal_F_000 372
_exptl_crystal_size_max 0.334
_exptl_crystal_size_mid 0.077
_exptl_crystal_size_min 0.047
_refine_diff_density_max 0.800
_refine_diff_density_min -0.392
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 172
_refine_ls_number_reflns 3617
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0234
_refine_ls_R_factor_gt 0.0209
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.1682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0532
_refine_ls_wR_factor_ref 0.0542
_reflns_number_gt 3348
_reflns_number_total 3617
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wp3011sup1.cif
_cod_data_source_block 9
_cod_depositor_comments
'Adding full bibliography for 2022286--2022290.cif.'
_cod_original_cell_volume 682.06(13)
_cod_database_code 2022288
_cod_database_fobs_code 2022288
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.490
_shelx_estimated_absorpt_t_max 0.892
_shelx_hkl_file
;
-4 -5 2 314.15 3.88
-4 -5 3 57.20 2.04
-4 -5 6 26.16 1.88
-4 -5 7 265.50 3.86
-3 -2 5 611.04 4.54
-3 -2 6 14.16 1.88
-3 -2 7 441.43 3.98
-2 -13 -14 86.46 3.48
-2 -2 13 53.99 2.94
-1 0 13 295.35 3.62
-1 1 10 528.64 4.17
0 -14 -16 165.25 3.58
0 1 13 46.25 2.27
1 -14 -16 51.10 2.58
1 2 10 622.28 5.27
2 -7 -10 4.11 1.66
3 -9 -11 56.24 2.01
3 -8 -10 6.09 1.87
3 -7 -9 342.92 3.56
3 -3 -4 321.10 3.69
4 -5 -5 0.68 1.55
4 -1 3 92.46 3.39
5 -3 3 2.27 2.96
-5 -10 -2 28.26 3.33
-5 -9 0 48.09 3.69
-4 -5 8 27.82 3.05
-3 -3 11 1.08 1.81
-3 -2 4 178.50 2.99
-3 -2 9 89.48 2.52
-2 -1 12 164.18 3.04
-2 0 6 6.35 1.59
-2 0 7 141.02 2.25
-2 0 8 224.37 2.88
-2 0 9 610.44 4.28
-1 -15 -16 94.63 3.69
-1 -12 -14 127.23 3.14
-1 -1 -1 462.24 9.82
-1 -1 15 46.16 2.81
-1 1 5 862.67 6.08
-1 1 11 19.82 1.94
0 -10 -13 66.23 1.90
0 -5 -8 58.87 2.05
0 0 15 103.55 3.36
0 2 8 329.27 3.80
0 2 9 0.74 1.60
1 -13 -15 16.10 2.65
1 -10 -13 106.28 2.29
1 -9 -12 168.19 2.91
1 -5 -8 16.88 1.70
1 -2 -4 79.78 2.14
1 2 6 108.09 3.28
2 -3 -5 134.29 2.51
2 0 15 6.41 2.97
2 2 8 755.81 8.87
2 2 9 7.38 2.12
3 -12 -13 29.96 2.73
4 -10 -10 18.05 2.07
4 -9 -9 82.73 3.02
5 -6 -3 84.52 3.21
-5 -11 -4 40.29 3.54
-4 -5 1 -0.97 1.83
-3 -14 -13 23.58 3.54
-3 -4 -2 232.36 4.18
-3 -3 0 174.54 3.41
-3 -3 12 141.27 3.49
-3 -2 3 171.01 2.96
-3 -2 10 116.92 2.76
-2 -15 -15 3.83 3.10
-2 -12 -13 12.86 2.35
-2 -2 14 19.41 2.40
-2 -1 13 110.61 2.92
-2 0 5 530.06 4.38
-1 0 14 32.06 2.54
-1 1 12 402.08 3.80
0 -13 -15 42.18 2.58
0 -9 -12 15.85 1.49
0 -8 -11 328.60 3.72
0 -7 -10 392.21 4.04
0 -6 -9 1293.30 6.98
0 -1 -2 14.08 2.07
0 1 14 0.21 2.19
0 2 7 225.79 3.43
0 2 10 752.79 5.39
0 2 11 60.61 2.12
1 -8 -11 205.82 2.95
1 -6 -9 558.03 4.41
1 2 12 161.11 2.93
2 -11 -13 50.32 2.70
2 2 10 236.38 4.56
3 -4 -5 26.30 2.00
3 -2 -2 647.09 5.15
4 -4 -3 102.83 2.53
5 -8 -5 32.10 3.11
5 -7 -4 24.19 2.75
5 -5 -1 83.42 3.20
5 -4 1 53.58 3.05
-5 -10 -3 100.57 4.19
-5 -9 -1 14.09 3.16
-5 -8 2 92.02 3.58
-4 -8 -5 85.44 3.78
-4 -4 6 -1.64 1.67
-4 -4 7 61.98 2.73
-4 -4 8 36.32 2.65
-3 -2 11 5.21 2.49
-2 -3 -3 940.58 12.97
-1 -14 -15 2.90 2.64
-1 -11 -13 46.97 2.47
0 -15 -16 95.75 3.41
0 0 16 24.26 2.75
1 -12 -14 30.97 2.44
1 1 15 90.84 3.06
2 -13 -14 27.87 2.94
2 -10 -12 8.93 2.29
2 2 11 2.53 2.28
3 -10 -11 207.09 3.14
3 0 14 64.00 4.79
4 -11 -10 40.33 3.24
4 -5 -4 166.11 3.00
4 -3 -1 240.12 3.48
4 -2 1 301.88 4.26
-5 -8 1 1.77 2.75
-4 -5 0 363.35 4.31
-4 -4 9 31.82 2.99
-3 -2 2 239.15 3.32
-3 -2 12 153.40 3.19
-2 -11 -12 163.11 3.91
-2 -1 1 11.93 1.34
-2 0 4 628.96 4.70
-2 0 12 176.00 3.00
-1 -10 -12 435.53 4.85
-1 0 15 212.14 3.72
-1 1 4 1348.10 7.85
-1 1 13 49.40 2.43
0 1 15 221.13 3.93
0 2 6 8.49 1.54
0 2 12 258.14 3.07
1 -14 -15 2.72 2.73
1 -11 -13 -0.18 2.08
1 -3 -5 477.26 4.70
1 -1 -2 469.02 5.64
2 -9 -11 112.94 2.44
2 -8 -10 0.19 1.82
2 -2 -3 2.91 1.49
2 2 7 58.61 3.55
3 -9 -10 23.76 1.68
3 -8 -9 157.19 2.78
3 -7 -8 119.96 2.52
3 -6 -7 102.57 2.43
4 -10 -9 27.67 2.58
4 -6 -5 5.28 2.21
4 -1 4 123.47 3.88
5 -6 -2 4.07 1.91
5 -4 2 56.91 3.46
5 -3 5 1.70 3.33
-5 -9 -2 22.28 4.54
-5 -8 0 58.35 4.30
-5 -7 3 -1.24 3.19
-3 -5 -4 2.80 2.26
-3 -1 6 18.52 1.94
-3 -1 7 318.36 3.19
-3 -1 8 151.28 2.44
-3 -1 9 129.83 2.68
-3 -1 10 192.55 3.01
-2 -14 -14 92.92 3.54
-1 -5 -7 414.01 5.47
-1 0 1 80.72 2.95
0 -14 -15 2.41 2.71
0 -11 -13 12.53 2.14
0 2 13 161.99 2.91
2 -12 -13 133.22 3.00
2 2 12 35.14 2.35
3 -12 -12 5.61 1.95
3 -3 -3 19.91 1.43
4 -8 -7 -0.79 1.75
4 -7 -6 144.72 2.60
4 -4 -2 148.72 2.94
5 -8 -4 -1.64 3.02
-5 -11 -5 55.01 4.22
-5 -7 2 54.95 3.35
-4 -7 -4 19.12 2.63
-4 -3 6 17.82 2.28
-4 -3 7 123.52 2.99
-3 -1 5 4.35 1.32
-2 0 3 203.62 3.18
-2 1 8 78.97 2.10
-2 1 9 38.64 1.81
-2 1 10 219.16 3.00
-1 -13 -14 68.66 2.88
-1 -9 -11 92.38 2.47
-1 -6 -8 104.12 3.08
-1 2 9 149.38 2.41
-1 2 10 362.08 3.34
-1 2 11 159.55 2.69
0 1 16 3.06 2.86
0 2 14 11.99 2.19
1 -13 -14 264.49 3.75
1 2 5 750.78 9.11
1 2 14 6.84 1.93
2 -14 -14 0.99 2.64
2 -11 -12 1.55 2.17
2 -1 -1 143.13 3.14
2 2 13 130.13 3.88
3 -4 -4 191.17 3.03
4 -11 -9 -1.03 2.86
-5 -10 -4 1.82 3.32
-5 -8 -1 9.08 2.84
-5 -7 1 10.82 2.45
-4 -5 -1 87.88 2.80
-4 -4 1 7.56 1.77
-4 -3 4 182.04 3.06
-4 -3 5 284.79 3.31
-4 -3 9 50.88 2.39
-4 -3 10 173.17 3.55
-3 -1 4 405.88 4.03
-3 -1 12 30.32 2.64
-2 -9 -10 58.53 2.91
-2 0 14 -0.71 1.97
-2 1 7 717.97 4.56
-2 1 11 1.40 1.35
-2 1 12 321.77 3.44
-1 -15 -15 30.96 2.85
-1 -8 -10 543.22 5.04
-1 -7 -9 567.79 5.41
-1 1 15 126.79 3.11
-1 2 7 1260.33 6.65
-1 2 12 279.86 3.34
0 -13 -14 109.68 3.06
0 2 5 2911.14 13.03
1 -15 -15 73.34 2.73
1 -9 -11 116.87 2.48
1 -4 -6 101.36 2.16
2 -10 -11 154.58 2.84
2 0 1 622.30 7.20
3 -2 -1 80.66 2.35
4 -10 -8 60.55 3.06
4 -5 -3 70.86 2.46
5 -7 -2 -0.84 2.80
5 -4 3 15.36 2.89
-5 -6 4 5.29 3.06
-3 -3 -1 331.79 4.59
-3 -2 1 51.78 2.14
-3 -1 13 33.25 2.87
-2 -13 -13 2.35 2.43
-2 -8 -9 119.13 3.88
-2 0 15 196.11 3.91
-2 1 6 211.95 2.96
-2 1 13 17.07 2.18
-1 -12 -13 0.91 2.04
-1 1 3 1275.75 8.35
-1 2 13 102.96 2.19
0 -15 -15 -0.32 2.46
0 -9 -11 160.19 2.88
0 2 15 108.38 3.08
1 -12 -13 153.88 2.94
1 -8 -10 29.11 1.52
1 -7 -9 243.04 3.15
1 -6 -8 55.10 2.00
1 -5 -7 927.51 5.79
1 2 15 103.98 3.39
2 -13 -13 22.52 2.15
2 2 14 33.05 3.19
3 -12 -11 63.33 2.78
3 -9 -9 22.97 1.64
3 -7 -7 109.92 2.55
3 -6 -6 232.83 3.08
3 -5 -5 2.96 1.29
4 -9 -7 1.46 2.36
4 -8 -6 118.35 3.04
4 -6 -4 38.09 2.22
4 -1 5 46.78 3.13
-5 -9 -3 40.80 3.20
-5 -7 0 81.11 3.01
-5 -6 3 34.41 3.01
-4 -6 -3 189.26 4.16
-4 -3 3 73.58 2.46
-4 -2 8 23.33 2.38
-3 -12 -11 0.76 3.35
-3 -1 3 21.99 1.91
-3 0 7 710.67 4.72
-3 0 8 6.22 1.52
-3 0 9 148.82 2.35
-3 0 10 255.21 3.32
-3 0 11 22.44 2.28
-2 -15 -14 152.46 4.36
-2 -7 -8 257.98 5.19
-2 1 14 65.19 2.69
-1 1 16 44.82 2.47
-1 2 14 71.18 2.72
0 -12 -13 15.13 2.30
0 -5 -7 1282.53 7.61
0 3 9 644.45 4.99
0 3 10 265.11 3.41
0 3 11 22.63 1.87
0 3 12 198.71 2.98
1 -14 -14 50.49 2.63
1 3 10 214.80 3.33
1 3 11 173.72 3.00
1 3 12 283.26 3.63
2 -8 -9 440.12 3.77
4 -4 -1 74.22 2.47
5 -5 2 18.13 3.29
-5 -8 -2 54.99 3.51
-5 -6 2 63.79 2.96
-5 -5 5 80.93 3.20
-4 -2 6 9.11 2.12
-4 -2 7 304.21 3.36
-4 -2 9 117.83 2.69
-4 -2 10 9.91 2.81
-3 0 6 88.97 2.29
-2 1 5 803.20 5.13
-1 -14 -14 302.44 4.21
-1 2 15 78.31 2.76
0 -14 -14 62.07 3.14
0 -7 -9 27.01 1.49
0 -6 -8 107.32 2.44
0 1 2 14.97 2.14
0 2 16 40.13 2.28
0 3 13 305.23 3.50
1 -11 -12 13.85 1.54
1 3 9 1.24 1.45
1 3 13 349.27 4.00
2 -14 -13 112.84 3.13
3 -11 -10 9.96 1.73
4 -11 -8 68.79 2.62
4 -5 -2 15.56 2.03
5 -8 -2 5.32 2.97
5 -7 -1 28.58 2.71
5 -4 5 8.72 3.92
-5 -5 4 64.38 3.28
-4 -4 0 179.05 3.30
-4 -2 5 151.68 2.95
-3 -4 -3 355.16 5.85
-3 0 13 16.12 2.62
-2 -12 -12 149.38 3.61
-2 1 15 41.32 2.41
-2 2 9 202.11 2.76
-2 2 11 41.56 2.13
-2 2 12 110.83 2.49
-1 3 11 108.11 2.34
0 -11 -12 183.84 3.00
0 3 8 144.67 2.78
0 3 14 204.45 3.24
1 -15 -14 9.85 2.75
1 -13 -13 98.69 2.71
1 -10 -11 383.43 3.76
2 -11 -11 110.97 2.33
2 -2 -2 1013.44 7.00
3 -10 -9 136.91 2.49
4 -10 -7 5.42 1.92
4 -9 -6 45.93 2.61
4 -6 -3 112.87 2.80
-5 -7 -1 56.68 3.05
-5 -6 1 9.22 2.64
-4 -5 -2 107.52 3.33
-4 -2 4 28.31 2.10
-3 0 5 558.29 4.22
-2 2 8 227.59 2.88
-1 -13 -13 71.83 2.67
-1 -10 -11 320.93 3.96
-1 2 16 1.19 1.93
-1 3 9 618.08 4.55
-1 3 10 444.49 3.70
-1 3 12 216.74 2.72
-1 3 13 48.46 2.23
0 2 17 65.00 2.95
0 3 15 172.20 3.39
1 -9 -10 82.42 2.32
1 3 8 305.95 4.39
1 3 15 115.23 3.24
2 -13 -12 1.27 1.78
3 -9 -8 240.64 2.88
3 -5 -4 680.60 4.91
4 -12 -8 33.95 2.88
4 -8 -5 18.04 1.80
4 -1 6 142.85 4.59
5 -7 0 17.59 2.85
5 -5 3 -0.15 2.80
5 -4 6 46.08 4.34
-5 -4 6 10.86 3.01
-4 -1 7 69.54 2.38
-4 -1 8 56.08 2.63
-4 -1 9 66.37 2.88
-4 -1 10 69.70 3.09
-4 -1 11 43.88 2.87
-3 -14 -12 89.04 4.52
-3 -1 2 725.54 5.21
-3 1 11 -1.25 2.13
-3 1 12 265.36 3.44
-2 -14 -13 34.28 2.82
-2 1 4 322.74 3.53
-2 2 7 863.16 5.11
-2 2 14 182.20 2.83
-1 3 14 49.40 2.31
0 -15 -14 44.14 2.87
0 -13 -13 212.99 3.33
0 -10 -11 92.52 2.46
0 2 4 266.84 4.56
0 3 7 681.43 5.58
0 3 16 1.89 2.20
1 -14 -13 27.29 2.51
1 -12 -12 58.01 2.33
1 -3 -4 972.38 6.79
2 -9 -9 118.00 2.48
2 2 16 16.87 3.18
3 -11 -9 7.73 2.27
3 -7 -6 166.59 2.50
3 -6 -5 -0.49 1.28
4 -11 -7 3.14 2.54
4 -4 0 0.65 1.87
5 -8 -1 71.69 3.27
-5 -11 -6 6.63 4.56
-5 -10 -5 184.79 5.59
-5 -9 -4 23.58 3.59
-5 -6 0 165.47 3.67
-5 -4 5 27.27 2.89
-4 -3 1 46.19 2.20
-4 -2 3 1.21 1.87
-4 -1 6 94.43 2.62
-3 -11 -10 222.20 5.61
-3 0 4 429.10 4.08
-3 1 7 90.92 2.20
-3 1 13 12.33 1.88
-2 -11 -11 152.70 3.58
-2 2 15 164.66 2.94
-1 -9 -10 2.49 1.61
0 -2 -3 1381.83 11.25
1 -8 -9 1188.90 5.86
1 -7 -8 6.28 1.58
1 -4 -5 1577.12 8.10
1 3 16 9.93 2.86
2 -14 -12 11.48 2.36
2 -12 -11 197.88 2.77
2 3 11 305.54 4.92
2 3 12 209.97 4.27
4 -10 -6 17.54 2.55
4 -5 -1 120.12 2.82
4 -3 2 11.09 2.54
5 -5 4 41.15 3.35
-5 -8 -3 87.92 4.02
-4 -4 -1 65.78 2.80
-3 1 14 120.00 2.86
-2 2 6 15.43 1.66
-1 -12 -12 108.26 2.80
-1 3 16 15.98 2.61
0 -16 -14 103.32 3.51
0 -12 -12 75.21 2.52
0 -9 -10 234.61 3.23
0 3 17 29.00 3.11
0 4 13 19.50 1.80
1 -6 -7 401.39 3.88
1 -5 -6 132.14 2.62
2 -11 -10 0.21 1.95
2 -4 -4 164.84 2.61
2 2 6 313.54 11.36
2 3 13 158.17 3.64
3 -3 -1 224.56 3.29
4 -12 -7 4.61 2.64
4 -9 -5 34.71 1.92
4 -8 -4 21.47 2.21
4 -7 -3 37.88 2.51
4 -6 -2 5.46 2.02
4 -2 4 62.01 2.71
4 -1 7 0.22 3.12
5 -8 0 19.81 3.13
5 -7 1 4.07 2.64
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1 -12 -7 18.77 1.63
1 -8 -4 194.51 2.53
2 -15 -12 7.22 2.20
2 -14 -11 106.30 2.20
2 -11 -8 109.90 1.92
2 -7 -5 38.63 1.47
2 -5 -4 846.85 4.64
2 5 -3 872.41 12.23
3 -4 -6 113.97 2.15
3 1 -5 4.23 1.24
4 -6 -11 36.48 2.08
4 -4 -10 3.01 1.80
4 -3 -10 -0.59 1.97
4 0 -10 69.70 2.63
-5 -5 -4 19.08 1.95
-5 4 -4 47.29 2.30
-4 5 -2 81.27 1.71
-3 6 -1 290.69 2.55
-3 10 -5 30.60 2.20
-1 -13 -6 211.78 3.21
-1 6 0 8.03 0.92
-1 9 -2 97.04 2.11
-1 10 -3 -0.55 1.43
-1 11 -5 5.38 1.75
0 -11 -5 19.10 1.46
0 -8 -3 24.49 1.45
0 11 -6 60.28 2.84
1 9 -4 209.29 3.92
1 10 -6 100.03 3.37
3 -8 -8 102.86 1.78
3 -1 -5 466.69 3.80
3 2 -5 573.71 4.89
4 -8 -12 5.48 2.22
4 -5 -10 24.55 1.94
4 1 -10 66.66 2.77
-5 -9 -6 6.69 2.69
-5 -7 -5 38.49 2.28
-5 5 -5 16.87 1.93
-4 -8 -4 1.95 1.86
-4 4 -2 92.82 1.90
-4 6 -3 3.01 1.51
-4 8 -5 20.21 2.24
-3 7 -2 264.50 2.64
-3 9 -4 119.13 2.45
0 -4 -1 2.41 1.21
1 -10 -5 7.45 1.28
1 8 -3 414.68 5.34
2 -3 -3 262.09 2.76
3 -12 -11 61.59 1.85
3 -11 -10 7.66 1.66
3 -7 -7 109.90 1.79
3 -2 -5 78.59 1.66
4 -7 -11 181.93 2.52
4 -3 -9 101.35 2.43
4 -2 -9 194.20 2.60
4 -1 -9 148.52 2.70
4 0 -9 85.65 2.45
-5 -4 -4 0.22 1.42
-5 4 -5 3.96 1.93
-2 -12 -5 77.68 3.10
-2 -1 0 1102.85 6.93
-1 -12 -5 4.90 1.45
-1 -9 -3 34.87 1.75
-1 -5 -1 97.38 4.26
0 -16 -9 24.50 1.79
2 -8 -5 2.19 1.22
2 -6 -4 662.12 3.93
3 -9 -8 234.41 2.57
3 -3 -5 119.97 2.16
3 3 -5 325.86 4.05
4 -9 -12 0.83 1.73
4 -4 -9 187.18 2.51
4 1 -9 65.31 2.30
-5 -3 -4 97.24 2.17
-5 -2 -4 28.78 1.86
-5 1 -4 24.52 1.67
-4 -1 -2 0.05 1.33
-4 1 -2 20.73 1.45
-4 5 -3 13.67 1.10
-4 6 -4 7.78 1.56
-4 7 -5 6.86 1.84
-3 6 -2 4.88 1.25
-3 9 -5 23.24 1.92
-2 3 0 19.49 1.24
-2 10 -5 27.73 1.91
-1 7 -1 864.90 4.86
0 8 -2 24.06 1.38
1 -17 -11 33.93 2.14
1 -15 -9 6.72 1.37
1 -7 -3 8.94 1.19
1 10 -7 44.37 2.72
2 -11 -7 9.68 1.19
2 -4 -3 0.51 1.08
3 -13 -11 30.15 1.94
3 -12 -10 63.50 2.01
3 -8 -7 5.41 1.40
3 -4 -5 29.73 1.49
3 5 -6 17.84 2.43
4 -7 -10 12.91 1.45
4 -2 -8 6.98 1.70
4 -1 -8 1.00 1.55
-5 -10 -7 42.45 2.92
-5 -6 -5 41.99 2.07
-5 3 -5 1.75 1.63
-3 7 -3 4.37 1.47
0 10 -5 14.41 1.91
1 -9 -4 813.28 4.34
2 -10 -6 228.96 2.52
2 1 -2 1518.48 8.09
3 -11 -9 6.83 1.22
3 -10 -8 48.87 1.66
4 -8 -10 17.15 1.96
4 -6 -9 81.68 1.78
4 0 -8 9.08 1.66
4 3 -10 151.58 3.79
-5 -8 -6 30.56 2.20
-4 7 -6 10.37 1.76
-1 -16 -8 117.61 2.85
-1 -11 -4 20.84 1.70
-1 10 -5 3.00 1.44
0 -7 -2 386.66 3.81
1 10 -8 31.88 2.64
2 -15 -10 54.48 2.18
2 -14 -9 3.46 1.78
2 -9 -5 0.95 1.15
2 -7 -4 269.76 2.59
3 -5 -5 2.13 1.25
4 1 -8 53.71 2.21
-5 -5 -5 132.89 2.44
-5 1 -5 -0.39 1.42
-5 3 -6 50.36 1.95
-4 6 -5 13.86 1.28
1 -11 -5 27.51 1.49
2 -12 -7 6.88 1.45
2 -5 -3 225.90 2.33
4 -9 -10 9.93 1.90
-5 0 -5 0.60 1.08
-3 6 -3 28.21 1.11
4 -8 -9 2.45 1.26
4 -3 -7 19.79 1.27
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 69516
_shelx_res_file
;
TITL g68_a.res in P-1
g68.res
created by SHELXL-2018/3 at 14:49:38 on 02-Apr-2020
REM Old TITL G68 JODOPOCHODNA
REM SHELXT solution in P-1
REM R1 0.063, Rweak 0.009, Alpha 0.047, Orientation as input
REM Formula found by SHELXT: C14 I N2 O S
CELL 0.71073 4.4279 13.0767 13.441 61.622 86.203 85.241
ZERR 2 0.0005 0.0014 0.0014 0.007 0.009 0.009
LATT 1
SFAC C H I N O S
UNIT 28 22 2 4 2 2
EQIV $1 1-X,1-Y,2-Z
L.S. 20
PLAN 4
SIZE 0.334 0.077 0.047
TEMP -153.15
HTAB N2 O1
HTAB C22 S1
HTAB N1 S1_$1
BOND $H
list 4
MORE -1
fmap 2
acta
MERG 2
OMIT -2 58
OMIT -3 11 13
REM
REM
REM
WGHT 0.036500 0.168200
FVAR 0.43986
I1 3 1.541658 0.977221 0.303151 11.00000 0.02755 0.02270 =
0.01967 -0.00969 0.00314 -0.00760
S1 6 0.694410 0.636340 0.853771 11.00000 0.03716 0.02775 =
0.02047 -0.01575 0.00619 -0.01240
O1 5 0.422505 0.430206 0.684137 11.00000 0.03155 0.02442 =
0.01985 -0.01289 0.00419 -0.00644
N2 4 0.723795 0.600527 0.671109 11.00000 0.02195 0.01994 =
0.01946 -0.01154 0.00200 -0.00421
AFIX 43
H2 2 0.659541 0.556723 0.644375 11.00000 -1.20000
AFIX 0
N1 4 0.410011 0.487600 0.820666 11.00000 0.02178 0.02106 =
0.01985 -0.01242 0.00372 -0.00449
AFIX 43
H1 2 0.322999 0.474879 0.886008 11.00000 -1.20000
AFIX 0
C24 1 1.299698 0.845426 0.433729 11.00000 0.01963 0.01805 =
0.01778 -0.00690 0.00033 -0.00285
C21 1 0.926885 0.684026 0.597604 11.00000 0.01853 0.01722 =
0.01686 -0.00789 -0.00077 -0.00037
C23 1 1.190403 0.860149 0.525238 11.00000 0.02716 0.02083 =
0.02147 -0.01232 0.00071 -0.00473
AFIX 43
H23 2 1.243847 0.925496 0.531840 11.00000 -1.20000
AFIX 0
C22 1 1.002398 0.779751 0.607814 11.00000 0.02615 0.02194 =
0.02215 -0.01391 0.00309 -0.00394
AFIX 43
H22 2 0.926668 0.790207 0.670373 11.00000 -1.20000
AFIX 0
C11 1 0.125278 0.322908 0.850741 11.00000 0.01885 0.01793 =
0.01753 -0.00899 -0.00218 0.00018
C12 1 0.085682 0.239044 0.817043 11.00000 0.02322 0.02291 =
0.02072 -0.01224 -0.00023 -0.00296
AFIX 43
H12 2 0.183570 0.245258 0.749489 11.00000 -1.20000
AFIX 0
C1 1 0.612597 0.576675 0.774224 11.00000 0.02061 0.01840 =
0.02112 -0.01072 -0.00082 -0.00076
C25 1 1.232883 0.748014 0.424765 11.00000 0.02579 0.02198 =
0.01833 -0.01183 0.00184 -0.00150
AFIX 43
H25 2 1.314542 0.736362 0.363510 11.00000 -1.20000
AFIX 0
C26 1 1.045354 0.668364 0.506649 11.00000 0.02636 0.01887 =
0.02130 -0.01259 0.00000 -0.00220
AFIX 43
H26 2 0.996650 0.602062 0.500796 11.00000 -1.20000
AFIX 0
C10 1 0.328766 0.417298 0.777827 11.00000 0.01917 0.01786 =
0.01887 -0.00989 -0.00131 -0.00008
C14 1 -0.238500 0.137645 0.980320 11.00000 0.02554 0.02115 =
0.02286 -0.00823 0.00075 -0.00518
AFIX 43
H14 2 -0.361951 0.074328 1.024676 11.00000 -1.20000
AFIX 0
C16 1 -0.022034 0.313512 0.949415 11.00000 0.02692 0.02061 =
0.01846 -0.01017 -0.00007 -0.00252
AFIX 43
H16 2 0.000485 0.370853 0.972299 11.00000 -1.20000
AFIX 0
C15 1 -0.201661 0.220636 1.014438 11.00000 0.02859 0.02384 =
0.01942 -0.00996 0.00256 -0.00369
AFIX 43
H15 2 -0.299221 0.213934 1.082217 11.00000 -1.20000
AFIX 0
C13 1 -0.095124 0.146978 0.881369 11.00000 0.02965 0.02225 =
0.02610 -0.01442 -0.00014 -0.00501
AFIX 43
H13 2 -0.121186 0.090296 0.857955 11.00000 -1.20000
AFIX 0
HKLF 4
REM g68_a.res in P-1
REM wR2 = 0.0542, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0209 for 3348 Fo > 4sig(Fo) and 0.0234 for all 3617 data
REM 172 parameters refined using 0 restraints
END
WGHT 0.0365 0.1682
REM Highest difference peak 0.800, deepest hole -0.392, 1-sigma level 0.089
Q1 1 1.6895 0.9362 0.2590 11.00000 0.05 0.80
Q2 1 1.3970 1.0214 0.3413 11.00000 0.05 0.66
Q3 1 0.9921 0.6772 0.5491 11.00000 0.05 0.46
Q4 1 1.3890 1.0049 0.2831 11.00000 0.05 0.46
;
_shelx_res_checksum 70627
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I1 1.54166(3) 0.97722(2) 0.30315(2) 0.02325(5) Uani d 1 . .
S S1 0.69441(13) 0.63634(4) 0.85377(4) 0.02636(10) Uani d 1 . .
O O1 0.4225(3) 0.43021(12) 0.68414(11) 0.0242(3) Uani d 1 . .
N N2 0.7238(4) 0.60053(13) 0.67111(13) 0.0195(3) Uani d 1 . .
H H2 0.659541 0.556723 0.644375 0.023 Uiso calc 1 . .
N N1 0.4100(4) 0.48760(13) 0.82067(13) 0.0198(3) Uani d 1 . .
H H1 0.322999 0.474879 0.886008 0.024 Uiso calc 1 . .
C C24 1.2997(4) 0.84543(15) 0.43373(15) 0.0191(3) Uani d 1 . .
C C21 0.9269(4) 0.68403(15) 0.59760(14) 0.0176(3) Uani d 1 . .
C C23 1.1904(4) 0.86015(16) 0.52524(16) 0.0221(3) Uani d 1 . .
H H23 1.243847 0.925496 0.531840 0.026 Uiso calc 1 . .
C C22 1.0024(4) 0.77975(16) 0.60781(16) 0.0220(3) Uani d 1 . .
H H22 0.926668 0.790207 0.670373 0.026 Uiso calc 1 . .
C C11 0.1253(4) 0.32291(15) 0.85074(14) 0.0178(3) Uani d 1 . .
C C12 0.0857(4) 0.23904(16) 0.81704(16) 0.0214(3) Uani d 1 . .
H H12 0.183570 0.245258 0.749489 0.026 Uiso calc 1 . .
C C1 0.6126(4) 0.57668(15) 0.77422(15) 0.0195(3) Uani d 1 . .
C C25 1.2329(4) 0.74801(16) 0.42476(15) 0.0212(3) Uani d 1 . .
H H25 1.314542 0.736362 0.363510 0.025 Uiso calc 1 . .
C C26 1.0454(4) 0.66836(16) 0.50665(15) 0.0209(3) Uani d 1 . .
H H26 0.996650 0.602062 0.500796 0.025 Uiso calc 1 . .
C C10 0.3288(4) 0.41730(15) 0.77783(15) 0.0182(3) Uani d 1 . .
C C14 -0.2385(5) 0.13765(17) 0.98032(16) 0.0239(4) Uani d 1 . .
H H14 -0.361951 0.074328 1.024676 0.029 Uiso calc 1 . .
C C16 -0.0220(4) 0.31351(16) 0.94942(15) 0.0216(3) Uani d 1 . .
H H16 0.000485 0.370853 0.972299 0.026 Uiso calc 1 . .
C C15 -0.2017(5) 0.22064(17) 1.01444(16) 0.0241(4) Uani d 1 . .
H H15 -0.299221 0.213934 1.082217 0.029 Uiso calc 1 . .
C C13 -0.0951(5) 0.14698(17) 0.88137(17) 0.0246(4) Uani d 1 . .
H H13 -0.121186 0.090296 0.857955 0.030 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
I1 0.02755(7) 0.02270(7) 0.01967(7) -0.00760(4) 0.00314(4) -0.00969(5)
S1 0.0372(3) 0.0277(2) 0.0205(2) -0.01240(19) 0.00619(18) -0.01575(18)
O1 0.0316(7) 0.0244(6) 0.0199(6) -0.0064(5) 0.0042(5) -0.0129(5)
N2 0.0220(7) 0.0199(7) 0.0195(7) -0.0042(6) 0.0020(6) -0.0115(6)
N1 0.0218(7) 0.0211(7) 0.0199(7) -0.0045(6) 0.0037(6) -0.0124(6)
C24 0.0196(8) 0.0181(7) 0.0178(7) -0.0028(6) 0.0003(6) -0.0069(6)
C21 0.0185(8) 0.0172(7) 0.0169(7) -0.0004(6) -0.0008(6) -0.0079(6)
C23 0.0272(9) 0.0208(8) 0.0215(8) -0.0047(7) 0.0007(7) -0.0123(7)
C22 0.0262(9) 0.0219(8) 0.0222(8) -0.0039(7) 0.0031(7) -0.0139(7)
C11 0.0188(8) 0.0179(7) 0.0175(7) 0.0002(6) -0.0022(6) -0.0090(6)
C12 0.0232(8) 0.0229(8) 0.0207(8) -0.0030(7) -0.0002(6) -0.0122(7)
C1 0.0206(8) 0.0184(7) 0.0211(8) -0.0008(6) -0.0008(6) -0.0107(6)
C25 0.0258(9) 0.0220(8) 0.0183(8) -0.0015(7) 0.0018(6) -0.0118(7)
C26 0.0264(9) 0.0189(8) 0.0213(8) -0.0022(7) 0.0000(7) -0.0126(7)
C10 0.0192(8) 0.0179(7) 0.0189(7) -0.0001(6) -0.0013(6) -0.0099(6)
C14 0.0255(9) 0.0211(8) 0.0229(8) -0.0052(7) 0.0007(7) -0.0082(7)
C16 0.0269(9) 0.0206(8) 0.0185(8) -0.0025(7) -0.0001(7) -0.0102(7)
C15 0.0286(9) 0.0238(8) 0.0194(8) -0.0037(7) 0.0026(7) -0.0100(7)
C13 0.0297(10) 0.0223(8) 0.0261(9) -0.0050(7) -0.0001(7) -0.0144(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.0390
0 -1 -1 0.0210
0 1 0 0.0430
0 -14 1 0.0360
17 6 -2 0.1330
-28 -10 -9 0.2560
0 6 29 0.0440
0 -7 -33 0.0460
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C21 N2 H2 . . 114.5 ?
C1 N2 H2 . . 114.5 ?
C1 N2 C21 . . 131.06(16) ?
C1 N1 H1 . . 115.7 ?
C10 N1 H1 . . 115.7 ?
C10 N1 C1 . . 128.66(15) ?
C23 C24 I1 . . 119.07(13) ?
C23 C24 C25 . . 120.57(17) ?
C25 C24 I1 . . 120.23(13) ?
C22 C21 N2 . . 124.91(16) ?
C22 C21 C26 . . 119.73(17) ?
C26 C21 N2 . . 115.30(15) ?
C24 C23 H23 . . 119.8 ?
C24 C23 C22 . . 120.46(17) ?
C22 C23 H23 . . 119.8 ?
C21 C22 C23 . . 119.28(17) ?
C21 C22 H22 . . 120.4 ?
C23 C22 H22 . . 120.4 ?
C12 C11 C10 . . 116.82(16) ?
C16 C11 C12 . . 119.22(17) ?
C16 C11 C10 . . 123.95(16) ?
C11 C12 H12 . . 119.8 ?
C13 C12 C11 . . 120.50(17) ?
C13 C12 H12 . . 119.8 ?
N2 C1 S1 . . 128.09(15) ?
N2 C1 N1 . . 114.60(16) ?
N1 C1 S1 . . 117.28(13) ?
C24 C25 H25 . . 120.6 ?
C26 C25 C24 . . 118.89(16) ?
C26 C25 H25 . . 120.6 ?
C21 C26 H26 . . 119.5 ?
C25 C26 C21 . . 121.00(16) ?
C25 C26 H26 . . 119.5 ?
O1 C10 N1 . . 122.06(17) ?
O1 C10 C11 . . 121.19(16) ?
N1 C10 C11 . . 116.74(15) ?
C15 C14 H14 . . 119.9 ?
C15 C14 C13 . . 120.15(18) ?
C13 C14 H14 . . 119.9 ?
C11 C16 H16 . . 119.9 ?
C15 C16 C11 . . 120.28(17) ?
C15 C16 H16 . . 119.9 ?
C14 C15 C16 . . 119.97(17) ?
C14 C15 H15 . . 120.0 ?
C16 C15 H15 . . 120.0 ?
C12 C13 C14 . . 119.86(18) ?
C12 C13 H13 . . 120.1 ?
C14 C13 H13 . . 120.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 C24 . 2.0930(18) ?
S1 C1 . 1.6656(19) ?
O1 C10 . 1.236(2) ?
N2 H2 . 0.8800 ?
N2 C21 . 1.413(2) ?
N2 C1 . 1.336(2) ?
N1 H1 . 0.8800 ?
N1 C1 . 1.400(2) ?
N1 C10 . 1.375(2) ?
C24 C23 . 1.384(2) ?
C24 C25 . 1.392(3) ?
C21 C22 . 1.392(2) ?
C21 C26 . 1.395(2) ?
C23 H23 . 0.9500 ?
C23 C22 . 1.394(3) ?
C22 H22 . 0.9500 ?
C11 C12 . 1.398(2) ?
C11 C10 . 1.488(2) ?
C11 C16 . 1.394(2) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.384(3) ?
C25 H25 . 0.9500 ?
C25 C26 . 1.385(3) ?
C26 H26 . 0.9500 ?
C14 H14 . 0.9500 ?
C14 C15 . 1.388(3) ?
C14 C13 . 1.391(3) ?
C16 H16 . 0.9500 ?
C16 C15 . 1.389(3) ?
C15 H15 . 0.9500 ?
C13 H13 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2 O1 . 0.88 1.87 2.620(2) 141.9 yes
N1 H1 S1 2_667 0.88 3.08 3.8864(17) 152.8 yes
C22 H22 S1 . 0.95 2.54 3.200(2) 126.3 yes